Charge preparation



" Patented an. 15,1946

CHARGE PREPARATIQN Robert K. Waring, Palmer-ton, Pa assignor to The New Jersey Zinc Company, New York, N. Y a corporation of New Jersey No Drawing. Application March 10, 1944, 4 Serial No. 525,970

1 (Cl. 7M7) This invention relates to charge preparation and more particularly to the preparation of a briquetted charge of calcined dolomite and ferrosilic'on for use in the production of magnesium. The invention contemplates an improvement in the wet briquetting of such a charge. More generally the invention contemplates an improvement in the calcination of dolomite or equivalent magnesium-bearing material.

In the production of magnesium by pyrometallurgical reduction or smelting of magnesium omde (magnesia) in calcined dolomite (or equivalent magnesiferous'material) by ferrosilicon (or equivalent reducing agent), it is customaryto briquet the mix (magnesiferous material and redueing agent). In a particularly advantageous wet process of briquetting the mix (disclosed in the copending patent application of Messrs. Wag

ner, Fetterolf, Waring and Mahler, Ser. No. 525,-969 filed Mar. 10, 1944), the calcined dolomite (calcine) is slacked with suflicient water to provide water of hydration and to provide free water to-yield a plastic mix of good briquetting consistency. The plastic mix is preferably densifled,

and then briquetted (or otherwise appropriately agglomerated), dried 'at a temperature of 100-110 0., and dehydrated (calcined) at a temperature of 650-750 C. Pillow-block shaped briquets about 2 inches by 2 inches by 1% inch are now commonly used in magnesium smelt- I have discovered that a calcined dolomite containing inactive magnesia that does not hydrate when moistened with water can be obtained, even from highly crystalline dolomite, by

adding calcium chloride to the dolomite either before calcination or during an early stage of calcination. I have further discovered that calwater which comprises carrying out the calcinaing in metal retorts about 10 inches internal diameter with about 5 feet of the retort length externally heated to a temperature 01' 1l50-1250 C. It is desirable that the briquets be as dense as possible in order to increase the weight of charge that can be introduced into the reducing retorts, thereby increasing the yield of magnesium per retort per cycle, the operating being of the intermittent or batch type. f

In the aforementioned wet process of briquetting the mix, the hydration of the calcium oxide (lime andmagnesium oxide in the calcine decreases the density of, the briquets after drying and dehydration. In the case of certain dolomites, particularly those that are highly crystalline, both the lime and magnesia in the calcined dolomite are hydrated (i. e.'convertedto calcium hydrate or hydroxide and magnesium hydrate .or hydroxide) when moistened with sufflcient water. The briquets obtained from such calcined .dolomites are of relatively low density say from 1.35 to 1.4 grams per 00., as compared with briquet \ide iiities of 1.65 .to 1.! obtained with calcineddolomitTirr which only the lime, and little or no magnesla, hydrates.

'tion in the presence of calcium chloride. More especially the invention contemplates the improvement in the aforementioned wet process of briquetting a mixture 'oi calcined dolomite and ferrcsilicon, which comprises calcining the dolomite in the presence of calcium chloride or sodium chloride. The agent (calcium chloride or sodium chloride) may be added to the dolomite before calcination or during the early stages of calcination, in amount of from 0.25;,to 1% by weight based on the weight of the calcine, or

from about 0.1 to about 0.5% based on the weight I.

of the stone (unealcined dolomite) The calcium chloride or sodium chloride may be advantageously added to the dolomite in the form of an aqueous solution sprayed on the stone before calcination. Either chloride may, however, be added in dry form to the dolomite. In order to obtain the best results it is desir able to hold to aminimum the water of plasticity, that isthe water added in excess of that required for hydration in order to impart suflicient plasticity to the mix for briquetting. Thus, in practice much higher densities have been obtained with 8% water of plasticity than with 13% the percentage figures being the quotient obtained by dividing. the weightof the water lost in drying the wet briquets (at a temperature of 100-110" C.) by the initial weight of the wet briquets.

m the case of sodium chloride, about 'to of'the chloride is 'volatilized during calcination. In general, the use of calcium chloride is to be preferred since calcium chloride almost completely inhibits the hydration of magnesia whileuthe inhibition brought about by sodium chloride is only partial.

The following table gives two practical examples oi the invention contrasted with wetbriquetting oi the same dolomite calcined in the absence 0! either sodium chloride or calcium chloride:

The percent or water lost in dehydration is the quotient obtained by dividing the weight of water lost in dehydrating the dried hydrated briquets (at a temperature of 650-750" C.) by the initial weight oi the dried briquets, and thus measures the amoimt of hydration.

The briquets were prepared by the hereinbeiore .mentloned process of wet briquetting, and contained stoichiometric equivalents of silicon (in the ierrosilicon) and magnesia (in the calcine), namely 28 parts silicon by weight per 80 parts magnesia by weight. They were dried at a temperature of 100-110" C. to remove the water of plasticity, and then heated or calcined at a temperature of 650-750 C. to remove the water of hydration. When the briquets (of the hereinbe- 2,sas,cao

before mentioned almond-shape) made from dolomite calcined in the presence of either calcium chloride or sodium chloride were reduced by the customary magnesium smelting process, the reduction and condensation of magnesium vapor proceeded as usual and neither the sodium chloride nor the calcium chloride had any harmful effect on the reaction.

It will be understood that the hydrated plastic mix may be formed into agglomerates by methods other than briquetting. as tor example by extrusion etc. For convenience such methods of aaglomerating are herein included under briquettins.

I claim:

A method ot'preparing briquets oi calcined dolomite and ierrosilicon, comprising calcining the dolomite, in admixture with a compound aelected from the group consisting oi calcium chloride and sodium chloride, slacking the calcined dolomite with suiiicient water to provide water of hydration at least for the calcium oxide and vsuiiflcient free waterto yield a plastic mix', the

said compound eflecting a substantially complete inhibition of the hydration of the magnesia whereby less water is required to form the plastic mix, mixing the slacked dolomite with ground ferrosilicon, briquetting the resulting mixture of slacked dolomite and terrcsilicon, and dehydrating the briquets.

ROBERT K. WARIN G. 

